CN110257627A - A kind of method that gold sulphide concentrate removes antimony, lead - Google Patents

A kind of method that gold sulphide concentrate removes antimony, lead Download PDF

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Publication number
CN110257627A
CN110257627A CN201910610617.8A CN201910610617A CN110257627A CN 110257627 A CN110257627 A CN 110257627A CN 201910610617 A CN201910610617 A CN 201910610617A CN 110257627 A CN110257627 A CN 110257627A
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CN
China
Prior art keywords
hydrogen peroxide
gold
antimony
hydrochloric acid
sulphide concentrate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910610617.8A
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Chinese (zh)
Inventor
邝江华
李希山
阳振球
陈芳斌
陆桂文
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CHENZHOU MINING INDUSTRY Co Ltd HUNAN
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CHENZHOU MINING INDUSTRY Co Ltd HUNAN
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Priority to CN201910610617.8A priority Critical patent/CN110257627A/en
Publication of CN110257627A publication Critical patent/CN110257627A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/045Leaching using electrochemical processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/10Hydrochloric acid, other halogenated acids or salts thereof
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a kind of gold sulphide concentrates except the method for antimony, lead, and gold sulphide concentrate is immersed in aqueous hydrochloric acid solution, opens stirring, and hydrogen peroxide is added, and controls the current potential of the solution system in hydrogen peroxide adition process between 350~390mV;Stop that hydrogen peroxide is added after solution system current potential is stablized, and the reaction was continued 1 hour or more for stirring;It is filtered after reaction, pickling, washing, obtains the gold sulphide concentrate except antimony, lead.This method is a kind of completely new technique, greatly reduces environmental pollution, eliminates the harm of mercury poison, and antimony, the removal rate of lead are high, Fen Bie ,≤99.5% of Wei≤99%, while the direct yield of gold has also been ensured, up to 99.5% or more.

Description

A kind of method that gold sulphide concentrate removes antimony, lead
Technical field
The invention belongs to field of smelting, are related to a kind of removal of high-grade gold sulphide concentrate antimony trisulfide, vulcanized lead, eliminate mercury poison Harm, and gold grade is improved, so that gold sulphide concentrate is entered the method for pyrogenic process purification.
Background technique
Antimony trisulfide, vulcanized lead impurity in high-grade gold sulphide concentrate, since antimony, lead have the ability for catching gold, pyrogenic process essence Refining removal of impurities cannot reach the separation of antimony, lead and gold.Be all made of after amalgamating is purified in the past and be sent to pyro-refining, mercury metal with Gold sulphide concentrate is mixed to get calomel, gold is separated with antimony, lead, calomel roasts output cake of gold, is used further to purify.Amalgamating Major drawbacks are that the health of serious damage operator is easy to pass through due to the extremely strong diffusivity of mercury and fat-soluble Human respiratory tract enters alveolar, generates harm to human body, operation in the environment for a long time be easy to cause mercury poisoning, and to environment It pollutes very big.
Summary of the invention
The purpose of the present invention is propose that a kind of both environmental protection, antimony lead are gone for the antimony trisulfide and vulcanized lead in gold sulphide concentrate Except rate height, social and economic benefits are obvious, and metal direct yield is high, and industrial truly feasible efficient from gold sulphide concentrate Except the method for antimony, lead.
The purpose of the present invention is to achieve the following:
A kind of method that gold sulphide concentrate removes antimony, lead, gold sulphide concentrate is immersed in aqueous hydrochloric acid solution, opens stirring, and Hydrogen peroxide is added, controls the current potential of the solution system in hydrogen peroxide adition process between 350~390mV;To solution system electricity Position stablizes (stablize in 350~390mV) and stops that hydrogen peroxide is added afterwards, and stirs that the reaction was continued 1 hour or more;It was carried out after reaction Filter, pickling, washing obtain the gold sulphide concentrate except antimony, lead.
Antimony trisulfide, vulcanized lead impurity in gold sulphide concentrate, which have, catches golden ability, therefore, how to realize antimony, lead it is efficient The direct yield for also guaranteeing good gold on the basis of removing is the technical issues of needing emphasis to solve.To solve this technical problem, The present inventor cooperates the rear reaction by numerous studies discovery, the potential value of the adding procedure of strict control hydrogen peroxide (the reaction was continued) can unexpectedly bring antimony, lead removal efficiency close to 100%, and the direct yield of gold is also close to 100% skill Art effect.
The present invention innovatively controls the current potential of hydrogen peroxide adding procedure, and further innovatively that potential value is accurate Ground controls in required range, moreover, the further cooperation rear reaction.Pass through the collaboration of the innovative technology Cooperation can unexpectedly realize the recycling of coupling antimony, the removing of lead and gold;The removing of antimony, lead nearly 100% may be implemented While, additionally it is possible to realize nearly 100% golden direct yield.
Preferably, the gold sulphide concentrate is high-grade gold sulphide concentrate.
Further preferably, the gold sulphide concentrate containing antimony be not higher than 5.0%, it is leaded to be not higher than 8.0%.
Preferably, the aqueous hydrochloric acid solution concentration is 4.5~5.5molL-1
Preferably, the ratio of the aqueous hydrochloric acid solution and gold sulphide concentrate is 5.5~7.5: 1.
Preferably, the addition time of hydrogen peroxide is not less than 0.5h.
The present invention initiatively controls the current potential of system in hydrogen peroxide adding procedure, and by current potential adding procedure Current potential is accurately controlled under required range, and so can be realized impurity additionally aids promotion gold while efficiently separating Direct yield.
Preferably, the current potential of the system in control hydrogen peroxide adition process is in 360~380mV.
The potentiometric electrode of the measurement solution potential device is reference electrode (calomel electrode) and platinum electrode.
3~7molL is filled in the calomel reference electrode outer tube-1Hydrochloric acid solution, it is molten that inner tube fills saturation potassium chloride Liquid.
The solution temperature for process that the reaction was continued after the completion of adding hydrogen peroxide and adding is 70~95 DEG C;Preferably 80~ 85℃。
The time that the reaction was continued after the completion of hydrogen peroxide addition is 1.5~5 hours.
The reaction carries out in whipping process, and mixing speed is 45~65r/min.
The washing process, pickling use dilute hydrochloric acid (3molL-1Left and right);Washing uses boiling water.
The utility model has the advantages that
The current potential that the present invention innovatively passes through hydrogen peroxide adding procedure is precisely controlled, further the cooperation rear reaction, The removal rate of antimony, lead can be effectively promoted, in addition, can also be obviously improved the direct yield of gold.
The study found that the removal rate of antimony is up to 99% or more, the removal rate of lead is up to 99.5% or more;
The direct yield of gold can reach 99.5% or more.
Detailed description of the invention
Fig. 1 is specific process flow chart of the invention:
Specific embodiment
Embodiment below is intended to illustrate invention rather than limitation of the invention further.The present invention can be with invention Any mode described in content is implemented.
The electrode of the potential measurement of case of the present invention is calomel reference electrode and platinum electrode;
3~7molL is filled in the calomel reference electrode outer tube-1Hydrochloric acid solution, it is molten that inner tube fills saturation potassium chloride Liquid.
Embodiment 1:
Gold 70.92% will be contained, contain antimony 1.05%, 5molL is added in leaded 5.14% gold sulphide concentrate-1Hydrochloric acid it is water-soluble In liquid, the ratio of aqueous hydrochloric acid solution and gold sulphide concentrate is 5.5: 1, is added and analyzes pure hydrogen peroxide progress control of Electric potentials, and control is double The current potential of the solution of oxygen water adding procedure stops addition hydrogen peroxide after 355~360mV stablizes up to current potential, continues thereafter with reaction 1.5 hours, 80 DEG C of temperature or so (± 2 DEG C) of the solution for process that hydrogen peroxide adds and the reaction was continued, the revolving speed of stirring was 45 ~65r/min.Then it filters, is washed 1 time with dilute hydrochloric acid, then 95 DEG C or more boiling water are cleaned.It obtains containing antimony containing gold 76.25% 0.052%, leaded 0.067% filter residue (gold sand).Antimony removal rate is 99.19%, and lead removal rate is 99.58%, golden direct yield It is 99.88%.
Embodiment 2:
Gold 53.67% will be contained, contain antimony 1.4%, 5.5molL is added in leaded 7.84% gold sulphide concentrate-1Hydrochloric acid water In solution, the ratio of aqueous hydrochloric acid solution and gold sulphide concentrate is 6: 1, is added and analyzes pure hydrogen peroxide progress control of Electric potentials, and control is double The current potential of the solution of oxygen water adding procedure stops addition hydrogen peroxide after 375~380mV stablizes up to current potential, continues thereafter with reaction 3 hours, 85 DEG C of temperature or so (± 2 DEG C) of the solution of hydrogen peroxide addition and the reaction was continued process, the revolving speed of stirring is 45~ 65r/min.Then it filters, is washed 1 time with dilute hydrochloric acid, then 95 DEG C or more boiling water are cleaned.It obtains containing antimony containing gold 73.16% 0.03%, leaded 0.024% filter residue (gold sand).Antimony removal rate is 99.37%, and lead removal rate is 99.69%, and golden direct yield is 99.82%.
Embodiment 3:
Gold 53.45% will be contained, contain antimony 1.5%, 5.5molL is added in leaded 6.2% gold sulphide concentrate-1Hydrochloric acid it is water-soluble In liquid, the ratio of aqueous hydrochloric acid solution and gold sulphide concentrate is 6.5: 1, is added and analyzes pure hydrogen peroxide progress control of Electric potentials, and control is double The current potential of the solution of oxygen water adding procedure stops addition hydrogen peroxide after 385~390mV stablizes up to current potential, continues thereafter with reaction 3.5 hours, 85 DEG C of temperature or so (± 2 DEG C) of the solution for process that hydrogen peroxide adds and the reaction was continued, the revolving speed of stirring was 45 ~65r/min.Then it filters, is washed 2 times with dilute hydrochloric acid, then 95 DEG C or more boiling water are cleaned.It obtains containing antimony containing gold 75.52% 0.017%, leaded 0.032% filter residue (gold sand).Antimony removal rate is 99.85%, and lead removal rate is 99.89%, golden direct yield It is 99.51%.
Comparison example 1:
Gold 51.61% will be contained, contain antimony 1.8%, 5.5molL is added in leaded 6.54% gold sulphide concentrate-1Hydrochloric acid water In solution, the ratio of aqueous hydrochloric acid solution and gold sulphide concentrate is 5.5: 1, is added and analyzes pure hydrogen peroxide progress control of Electric potentials, terminal Current potential stablize in 435~440mV, 85 DEG C of temperature or so, react 3 hours, then filter, wash 1 time, then 95 DEG C with dilute hydrochloric acid The above boiling water is cleaned.It obtains containing antimony 0.03%, leaded 0.024% filter residue (gold sand) containing gold 73.16%.Golden direct yield is 89.52%.
Comparison example 2:
Gold 51.61% will be contained, contain antimony 1.95%, 5.5molL is added in leaded 4.54% gold sulphide concentrate-1Hydrochloric acid water In solution, the ratio of aqueous hydrochloric acid solution and gold sulphide concentrate is 5.5: 1, and not plus hydrogen peroxide carries out control of Electric potentials, initial potential is- 103mv, reacts 3 hours by 85 DEG C of temperature or so, and current potential is -95mv after reaction.Then it filters, washs 1 time, then 95 with dilute hydrochloric acid DEG C or more boiling water clean.It obtains containing antimony 1.94%, leaded 4.55% filter residue containing gold 51.69%.Hydrogen peroxide is not added, substantially without Effect.
Comparison example 3:
Gold 48.62% will be contained, contain antimony 2.16%, 5.5molL is added in leaded 3.78% gold sulphide concentrate-1Hydrochloric acid water In solution, the ratio of aqueous hydrochloric acid solution and gold sulphide concentrate is 5.5: 1, is added and analyzes pure hydrogen peroxide progress control of Electric potentials, terminal Current potential stablize in 325-335mV, 85 DEG C of temperature or so, react 3 hours.Then it filters, washs 1 time, then 95 DEG C with dilute hydrochloric acid The above boiling water is cleaned.It obtains containing antimony 0.60%, leaded 0.92% filter residue containing gold 51.19%.Antimony removal rate is 72.22%, lead Removal rate is 55.82%, and golden direct yield is 75.66%.

Claims (10)

1. a kind of gold sulphide concentrate is except the method for antimony, lead, which is characterized in that immerse in aqueous hydrochloric acid solution gold sulphide concentrate, open Stirring is opened, and hydrogen peroxide is added, controls the current potential of the solution system in hydrogen peroxide adition process between 350~390mV;To molten Liquid system current potential stops that hydrogen peroxide is added after stablizing, and the reaction was continued 1 hour or more for stirring;It is filtered after reaction, pickling, water It washes, obtains the gold sulphide concentrate except antimony, lead.
2. the method according to claim 1, wherein the gold sulphide concentrate containing antimony be not higher than 5.0%, it is leaded Not higher than 8.0%.
3. the method according to claim 1, wherein aqueous hydrochloric acid solution concentration is 4.5~5.5molL-1
4. the method according to claim 1, wherein the ratio of aqueous hydrochloric acid solution and gold sulphide concentrate be 4.5~ 7.5∶1。
5. the method according to claim 1, wherein the addition time of hydrogen peroxide is not less than 0.5h.
6. the method according to claim 1, wherein the current potential of the system in control hydrogen peroxide adition process exists 360~380mV.
7. method according to claim 1 or 6, which is characterized in that measurement solution potential device potentiometric electrode be Calomel reference electrode and platinum electrode;
3~7molL is filled in the calomel reference electrode outer tube-1Hydrochloric acid solution, inner tube fill saturated potassium chloride solution.
8. the method according to claim 1, wherein the reaction was continued mistake after the completion of addition hydrogen peroxide and addition The solution temperature of journey is 70~95 DEG C.
9. according to the method described in claim 8, it is characterized in that, the time that the reaction was continued after the completion of hydrogen peroxide addition is 1.5 ~5 hours.
10. the method according to claim 1, wherein mixing speed is 45~65r/min;
Washing process pickling uses dilute hydrochloric acid;Washing uses boiling water.
CN201910610617.8A 2019-07-08 2019-07-08 A kind of method that gold sulphide concentrate removes antimony, lead Pending CN110257627A (en)

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Application publication date: 20190920